Ambavaram Vijaya Bhaskar Reddy, Nandigam Venugopal, Vemula Madhavi, Kalluru Gangadhara Reddy, Gajulapalle Madhavi
Sri Venkateswara University, Department of Chemistry, Tirupati, A.P., 517502, India.
Biomed Chromatogr. 2013 Jul;27(7):916-23. doi: 10.1002/bmc.2882. Epub 2013 Mar 6.
A sensitive and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for simultaneous determination of urapidil and aripiprazole in human plasma. A simple liquid-liquid extraction with ethyl acetate was used for the sample preparation. Chromatographic separation was achieved on a Phenomenex C18 (4.6 × 50 mm, 5 µm) column with 0.1% formic acid-acetonitrile (10:90, v/v) as the mobile phase with flow rate of 0.6 mL/min. The quantitation of the target compounds was determined in a positive ion multiple reaction monitoring mode. Calibration plots were linear over the range of 2.0-2503.95 ng/mL for urapidil and 1.0-500.19 ng/mL for aripiprazole. The lower limit of quantitation for urapidil and aripiprazole was 2.0 and 1.0 ng/mL, respectively. Mean recovery was in the range of 69.94-75.62% for both analytes and internal standards. Intra-day and inter-day precisions of the assay at three concentrations were 2.56-5.89% with accuracy of 92.31-97.83% for urapidil, and 3.14-6.84% with accuracy of 91.38-94.42% for aripiprazole. The method was successfully applied to human pharmacokinetic study of urapidil and aripiprazole in healthy human male volunteers.
建立了一种灵敏且选择性好的液相色谱 - 串联质谱（LC-MS/MS）方法，并进行了验证，用于同时测定人血浆中的乌拉地尔和阿立哌唑。采用简单的乙酸乙酯液 - 液萃取法进行样品制备。在Phenomenex C18（4.6×50 mm，5 µm）色谱柱上进行色谱分离，以0.1%甲酸 - 乙腈（10:90，v/v）为流动相，流速为0.6 mL/min。在正离子多反应监测模式下测定目标化合物的定量。乌拉地尔的校准曲线在2.0 - 2503.95 ng/mL范围内呈线性，阿立哌唑的校准曲线在1.0 - 500.19 ng/mL范围内呈线性。乌拉地尔和阿立哌唑的定量下限分别为2.0和1.0 ng/mL。两种分析物和内标的平均回收率在69.94% - 75.62%范围内。该方法在三个浓度下的日内和日间精密度，乌拉地尔为2.56% - 5.89%，准确度为92.31% - 97.83%；阿立哌唑为3.14% - 6.84%，准确度为91.38% - 94.42%。该方法成功应用于健康男性志愿者中乌拉地尔和阿立哌唑的人体药代动力学研究。
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